CN103739944A - Low-odour glass-fiber-enhanced polypropylene composite material and preparation method thereof - Google Patents
Low-odour glass-fiber-enhanced polypropylene composite material and preparation method thereof Download PDFInfo
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- CN103739944A CN103739944A CN201310660155.3A CN201310660155A CN103739944A CN 103739944 A CN103739944 A CN 103739944A CN 201310660155 A CN201310660155 A CN 201310660155A CN 103739944 A CN103739944 A CN 103739944A
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
- C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L23/10—Homopolymers or copolymers of propene
- C08L23/14—Copolymers of propene
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
- B29B9/00—Making granules
- B29B9/12—Making granules characterised by structure or composition
- B29B9/14—Making granules characterised by structure or composition fibre-reinforced
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- B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
- B29B7/00—Mixing; Kneading
- B29B7/30—Mixing; Kneading continuous, with mechanical mixing or kneading devices
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B29C48/04—Particle-shaped
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- C08J9/04—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent
- C08J9/12—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a physical blowing agent
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Abstract
The invention discloses a low-odor glass-fiber-enhanced polypropylene composite material comprising the following components: 37-83% of polypropylene resin, 2-10% of a compatilizer, 5-40% of glass fiber, 0-20% of a mineral filler, 0.5-5% of jellyfish grains and 0.1-3% of an assistant; the preparation method is as follows: mixing the polypropylene resin, the compatibilizer, the mineral filler and the assistant in a high mixing machine for 1-3min; evenly mixing, putting the mixture into a main feeding port of a double screw extruder, adding the jellyfish grains from a side feeding port, and then adding the glass fiber from the side feeding port of the extruder for melt extrusion and drying granulation to obtain the low-odor glass-fiber-enhanced polypropylene composite material. The low-odor glass-fiber-enhanced polypropylene composite material uses the jellyfish grains, using high-melt foaming PP (polypropylene) as a carrier, as a stripping agent for effective removal of various volatile small molecules and organic compounds produced in the machining process, and the prepared glass-fiber-enhanced polypropylene composite material has the characteristics of low odor, excellent mechanical properties and the like.
Description
Technical field
The present invention relates to a kind of glass fiber reinforced polypropylene composite material, be specifically related to a kind of low smell glass fiber reinforced polypropylene composite material and preparation method thereof.
Background technology
Fiber glass reinforced polypropylene has the advantages such as physical strength is high, good heat resistance, resistance to chemical attack, dimensional stabilizing, is widely used in the fields such as household electrical appliance, automobile, machinery.The strength and modulus of the fiber glass reinforced polypropylene engineering plastics that can match in excellence or beauty, this has further expanded the application prospect of Reinforced Polypropylene.Be applied to the glass fiber material of automotive upholstery in application process, except requiring to have good mechanical property, processing characteristics, weather resistance, also will have good low volatility, wherein smell requirement is that volatile matter one of is evaluated.
The reason that fiber glass reinforced polypropylene material smell produces is many-sided.First, the initiator that matrix acrylic resin is used in building-up process and catalyst system itself contain the compound of pungent odour, and, polypropylene matrix is in carrying out the process of modification, can there is autoxidation degraded in the polypropylene of molten state, produce some low molecular compound, and these materials are included in the material after modification, in the use procedure of molded article and product, come out, produce more smell.Secondly, the phase solvent component in composite glass fiber Reinforced Polypropylene material is generally used some anhydrides graftss, and the small molecules in itself and grafting process also has irritating smell.Moreover the alkali-free glass fiber in fiber glass reinforced polypropylene material also can contain some is with impurity odorous, simultaneously in order to meet various requirement, often add the materials such as mineral filler, elastomerics, oxidation inhibitor, damage resistant agent.These materials also can produce volatile matter in the course of processing.If smell is large, will severe contamination car in air, affect the healthy of driver and crew.
Reduce smell and can take several measures below: 1, by low smell substitute, substitute those unpleasant additives; 2, adopt more pure resin; 3, add sorbent material, comprise chemical reaction and physical adsorption method.Chemical reaction method refers to the additive that some can react with scent of small-molecule substance, these additives and small molecules reaction, produce the another kind of compound that molecular chain is large, can not evaporate in general environment, thereby elimination smell, for example zinc ricinate reduces smell by chelating aldehyde ketone molecule.And for physical adsorption, theoretically, a large amount of cavities can be adsorbed the small molecules of any generation smell or other fugitive constituents, and conventional physical absorbent comprises gac, silica gel, Attapulgite, clay mineral system, molecular sieve, zeolite, wollastonite, wilkinite etc. at present.
It is that resinogen material, stablizer, mineral filler and processing cracking produce that patent 200510026760.0 is mentioned smell, smell solution: nano zine oxide and nano titanium oxide.Patent CN101817953B has added odor adsorption agent and has prepared a kind of low modified polypropylene composite material distributing, and odor adsorption agent comprises: clay, wilkinite, porous silica, activated alumina or molecular sieve.Patent CN102030945A has added the glass strengthening matrix material that a kind of smell inhibitor is prepared a kind of low smell, and its smell inhibitor is zinc ricinate, and metal oxide and clay mineral are composite to be formed.
Aforesaid method to the smell problem of polypropylene material by solution in various degree, yet, aforesaid method is only the impact on smell for a certain component, reduce smell, but in fact inside gadget material smell is the interactional result of various ingredients smell thereby add sorbent material.Therefore, develop a kind of polypropylene composite material that can comprehensively solve various smell problems and seem particularly important.
Summary of the invention
In order to overcome the defect of above-mentioned prior art, primary and foremost purpose of the present invention is to provide a kind of low smell glass fiber reinforced polypropylene composite material, said composition is by adding jellyfish grain, can effectively remove the various volatile small molecule and the organic compound that in the course of processing, produce, not affect the mechanical property of material simultaneously.
Another object of the present invention is to provide a kind of preparation method of above-mentioned low smell glass fiber reinforced polypropylene composite material.
The present invention is achieved through the following technical solutions:
A low smell glass fiber reinforced polypropylene composite material, by weight percentage, comprises following component:
Acrylic resin 37-83%;
Compatilizer 2-10%;
Glass fibre 5-40%;
Mineral filler 0-20%
Jellyfish grain 0.5-5%;
Auxiliary agent 0.1-3%;
Wherein, described jellyfish grain by weight percentage, comprises following component:
Polypropylene 1%-49%;
Water 50%-98%;
Mineral filler 0.1-5%;
Jellyfish grain of the present invention, is by polypropylene, the mixture that mineral filler and water form, this mixture water content >=50%, preferably 60-90%.Described polypropylene is high melt strength, propylene, its melt strength >=5cN.Wherein, melt strength test condition is: under the experimental temperature of 190 ℃, use the capillary die that length-to-diameter ratio is 10:1, mouthful mould is 24cm to the distance of roller, and plunger lowering speed is 0.10mm/s, and the acceleration of traction rollers is 5mm/s
2.
The preparation method of described jellyfish grain, comprises the steps:
(1) polypropylene is mixed by proportioning fully with mineral filler, in forcing machine, extrude strip polypropylene, then be chopped into polypropylene pre-expanded particles;
(2) take water as whipping agent, polypropylene pre-expanded particles is foamed, prepare the expanded polypropylene of high fondant-strength;
(3) the mixed 5-10min in super mixer by the expanded polypropylene of high fondant-strength and water, prepares jellyfish grain, emits stand-by.
The preferred 0.5-5% of jellyfish grain add-on of the present invention, adds too much jellyfish grain, and jellyfish grain can seethe with excitement in screw rod, thereby is unfavorable for producing.
Described acrylic resin is one or more of homopolymerization PP and/or copolymerization PP, and its melt flow rate (MFR) is 1-90g/10min under 230 ℃, 2.16kg condition.
Described compatilizer is the grafts of polypropylene and unsaturated acid or unsaturated acid anhydride, and its percentage of grafting is 0.3-1.2%, and melting index is 50-120g/10min under 190 ℃, 2.16kg condition.Described unsaturated acid or unsaturated acid anhydride are one or more in toxilic acid, vinylformic acid, methylene-succinic acid, maleic anhydride, vinylformic acid Racemic glycidol fat.
Described glass fibre is one or more mixing of long glass fibres or short glass fiber.
Preferably, described long glass fibres is alkali free glass fibre, and diameter is 10-16 μ m; The length of described short glass fiber is 0.2-10mm, and diameter is 8-20 μ m.
Described mineral filler is one or more the mixture in talcum powder, calcium carbonate, barium sulfate.
The present composition also comprises 0.1-3%(weight percent) auxiliary agent, described auxiliary agent is one or more the mixing in thermo-stabilizer, photostabilizer, processing aid, toner or pigment.Because the present invention is automotive trim polypropene composition, can to above-mentioned auxiliary agent, use separately according to the structure of different automotive trims, technical requirements etc., or compound use.Thermo-stabilizer can improve the heat aging property of material in processing and use procedure, conventionally can be selected from more than one in phenols, phosphorous acid esters, monothioester class.Photostabilizer can improve material light aging resisting property in use, can be hindered amines or UV light absorber.Processing aid is more than one in low molecule ester class stearic acid, metallic soap (Cast, Znst), stearic acid complex ester or amides (erucicamide).
The preparation method of low smell glass fiber reinforced polypropylene composite material of the present invention, comprises the following steps:
(1) take by weight percentage acrylic resin, compatilizer, mineral filler and auxiliary agent and in high mixer, mix 1-3min; Mix, obtain Preblend;
(2) Preblend is placed in to the main spout of twin screw extruder, from side spout, adds jellyfish grain, glass fibre also, from the side spout feeding of forcing machine, melt extrudes, and granulating and drying, obtains.
The present invention compared with prior art, has following beneficial effect:
1) the present invention uses and to using jellyfish grain that high flux foaming PP is carrier as air lift agent, can effectively remove the various volatile small molecule and the organic compound that in the course of processing, produce, prepared glass fiber reinforced polypropylene composite material has low smell, characteristic that physical strength is high;
2) the jellyfish grain that the present invention uses is simple and easy to get, and preparation technology is simple, and cost is low, when can effectively remove smell, and
Do not affect the mechanical property of composition;
3) preparation method of the low smell glass fiber reinforced polypropylene composite material that the present invention proposes is simple, takes side feeding to feed in raw material
Mode adds jellyfish grain, has avoided adding problem fashionable and that cause the moisture jellyfish grain to volatilize too early from main feeding, can more effectively remove smell.
Embodiment
Below by embodiment, further illustrate the present invention, following examples are preferably embodiment of the present invention, but embodiments of the present invention are not subject to the restriction of following embodiment.
In following examples and comparative example, the processing conditions that forcing machine melt extrudes is as follows: a district temperature 210-230 ℃, two district temperature 220-240 ℃, three district temperature 220-240 ℃, four district temperature 220-240 ℃, five district temperature 230-250 ℃, six district temperature 240-260 ℃, seven district temperature 230-250 ℃, eight district temperature 220-240 ℃, nine district temperature 200-220 ℃, engine speed 250-600 rev/min.
Long glass fibres: be selected from the general roving glass fiber of megalith group, Fibre diameter is 13 μ m, and linear density is 2000tex, and model is ER13-2000-988A;
Short glass fiber: be selected from the glass 147A series that U.S. OCV company produces, the length of its glass fibre is 4mm, and diameter is 14 μ m.
the preparation of jellyfish grain:
The high melt strength, propylene of different melt intensity is mixed by proportioning shown in table 1 fully with mineral filler (talcum powder, calcium carbonate or barium sulfate), in forcing machine, extrude strip polypropylene, then be chopped into polypropylene pre-expanded particles; Take water as whipping agent, polypropylene pre-expanded particles is foamed, prepare the expanded polypropylene of high fondant-strength; The mixed 5-10min in super mixer by the expanded polypropylene of high fondant-strength and water, by controlling mixing time, prepares the jellyfish grain of water content as shown in table 1, emits stand-by.
Each component concentration (weight percent) of table 1 jellyfish grain
embodiment 1-5
A low smell glass fiber reinforced polypropylene composite material, its composition of raw materials is as shown in table 3, and its preparation method comprises the following steps:
(1) take by weight percentage polypropylene, compatilizer, mineral filler and auxiliary agent, in high mixer, mixed 1-3min; Mix, obtain Preblend;
(2) Preblend is placed in to the main spout of twin screw extruder, from side spout, adds jellyfish grain, glass fibre also, from the side spout feeding of forcing machine, melt extrudes granulating and drying.Its performance test is as shown in table 4.
Wherein, Co-polypropylene in embodiment 1: the AS164 (melt flow rate (MFR) (230 ℃/2.16kg) is 1.5g/10min) that is selected from Singapore's polyolefins company; Homo-polypropylene is selected from the EP540V (melt flow rate (MFR) (230 ℃/2.16kg) is 87g/10min) of Moplen.
Homo-polypropylene in embodiment 2: the HC9012-M (melt flow rate (MFR) (230 ℃/2.16kg) is 10g/10min) that is selected from China Petrochemical Industry Maoming.
In embodiment 3, Co-polypropylene is selected from the EP300M (melt flow rate (MFR) (230 ℃/2.16kg) is 10g/10min) of CSPC.
In embodiment 4, Co-polypropylene is selected from the HJ4045 (melt flow rate (MFR) (230 ℃/2.16kg) is 45g/10min) of Korea S's oiling.
In embodiment 5, Co-polypropylene is selected from the EP300M (melt flow rate (MFR) (230 ℃/2.16kg) is 10g/10min) of CSPC; Homo-polypropylene is selected from the HP550J (melt flow rate (MFR) (230 ℃/2.16kg) is 3g/10min) of CSPC.
comparative example 1
A glass fiber reinforced polypropylene composite material, its composition of raw materials is as shown in table 3, and its preparation method comprises the following steps:
(1) taken by weight percentage polypropylene, compatilizer, mineral filler, jellyfish grain and auxiliary agent mix 1-3min in high mixer; Mix, obtain Preblend;
(2) Preblend is placed in to the main spout of twin screw extruder, glass fibre, from the side spout feeding of forcing machine, melt extrudes granulating and drying.
comparative example 2
A glass fiber reinforced polypropylene composite material, its composition of raw materials is as shown in table 3, and its preparation method comprises the following steps:
(1) take by weight percentage polypropylene, compatilizer, mineral filler and auxiliary agent, in high mixer, mixed 1-3min; Mix, obtain Preblend;
(2) Preblend is placed in to the main spout of twin screw extruder, glass fibre, from the side spout feeding of forcing machine, melt extrudes granulating and drying.
comparative example 3
A glass fiber reinforced polypropylene composite material, its composition of raw materials is as shown in table 3, and its preparation method is with comparative example 2.
comparative example 4
A glass fiber reinforced polypropylene composite material, its composition of raw materials is as shown in table 3, and its preparation method is with embodiment 1.
The polypropylene composite material that embodiment and comparative example obtain adopts following methods to test its correlated performance:
(1) measurement of odor standard: by the VW ' s PV3900E of Volkswagen standard, adopt 1 ~ 6 grade of evaluation, rank is higher, and smell is larger.Concrete regulation is as table 2
VW ' s the PV3900E of table 2 Volkswagen standard
(2) mechanical property: test by following standard respectively
A tensile strength: press ISO527 test; Speed is 50mm/min;
B socle girder notched Izod impact strength: press ISO180 test;
C flexural strength, modulus in flexure: press ISO178 test, speed is 2mm/min;
D elongation at break: press ISO527 test.
The composition of raw materials of the polypropylene composite material of table 3 embodiment and comparative example (by weight percentage)
The performance data of the polypropylene composite material of table 4 embodiment and comparative example
By embodiment 2 and comparative example 2, embodiment 3 contrasts and can find out with comparative example 3, and adding of the jellyfish grain that the high flux foaming PP of take is carrier, can effectively remove various volatile small molecule and the organic compound in polypropylene composite material really.The present invention prepare glass fiber reinforced polypropylene composite material, there is low smell, feature that physical strength is high.
In addition, by embodiment 1 and comparative example 1 contrast, can be found out, comparative example 1 takes main feeding feed way to add jellyfish grain, and embodiment 1 takes the reinforced mode of side feeding, the better excellence of its effect; This is because adding membership from main feeding causes the moisture jellyfish grain to vapor away too early, affects its effect.
Embodiment 4 compares with comparative example 4, and the water content of comparative example 4 jellyfish grains is lower, and the glass fiber reinforced polypropylene composite material smell of preparation is poor.
Claims (13)
1. a low smell glass fiber reinforced polypropylene composite material, is characterized in that: by weight percentage, comprise following component:
Acrylic resin 37-83%;
Compatilizer 2-10%;
Glass fibre 5-40%;
Mineral filler 0-20%
Jellyfish grain 0.5-5%;
Auxiliary agent 0.1-3%;
Wherein, described jellyfish grain by weight percentage, comprises following component:
Polypropylene 1%-49%;
Water 50%-98%;
Mineral filler 0.1-5%;
Described polypropylene is high melt strength, propylene, its melt strength >=5cN.
2. low smell glass fiber reinforced polypropylene composite material according to claim 1, is characterized in that: described acrylic resin is one or more of homopolymerization PP and/or copolymerization PP, and its melt flow rate (MFR) is 1-90g/10min under 230 ℃, 2.16kg condition.
3. low smell glass fiber reinforced polypropylene composite material according to claim 1, it is characterized in that: described compatilizer is the grafts of polypropylene and unsaturated acid or unsaturated acid anhydride, its percentage of grafting is 0.3-1.2%, and melting index is 50-120g/10min under 190 ℃, 2.16kg condition.
4. low smell glass fiber reinforced polypropylene composite material according to claim 3, is characterized in that: described unsaturated acid or unsaturated acid anhydride are one or more in toxilic acid, vinylformic acid, methylene-succinic acid, maleic anhydride, vinylformic acid Racemic glycidol fat.
5. low smell glass fiber reinforced polypropylene composite material according to claim 1, is characterized in that: described glass fibre is one or more mixing of long glass fibres or short glass fiber.
6. low smell glass fiber reinforced polypropylene composite material according to claim 5, is characterized in that: described long glass fibres is alkali free glass fibre, and diameter is 10-16 μ m; The length of described short glass fiber is 0.2-10mm, and diameter is 8-20 μ m.
7. low smell glass fiber reinforced polypropylene composite material according to claim 1, is characterized in that: described mineral filler is one or more the mixture in talcum powder, calcium carbonate, barium sulfate.
8. low smell glass fiber reinforced polypropylene composite material according to claim 1, is characterized in that: described auxiliary agent is one or more the mixing in thermo-stabilizer, photostabilizer, processing aid, toner or pigment.
9. low smell glass fiber reinforced polypropylene composite material according to claim 8, is characterized in that: described thermo-stabilizer is more than one in phenols, phosphorous acid esters, monothioester class; Described photostabilizer is one or more the mixing in hindered amines or UV light absorber; Described processing aid is more than one in low molecule ester class stearic acid, metallic soap, stearic acid complex ester or amides.
10. low smell glass fiber reinforced polypropylene composite material according to claim 1, is characterized in that: in described jellyfish grain, water content is 60-90%.
11. low smell glass fiber reinforced polypropylene composite materials according to claim 1, is characterized in that: the preparation method of described jellyfish grain, comprises the steps:
(1) polypropylene is mixed by proportioning fully with mineral filler, in forcing machine, extrude strip polypropylene, then be chopped into polypropylene pre-expanded particles;
(2) take water as whipping agent, polypropylene pre-expanded particles is foamed, prepare the expanded polypropylene of high fondant-strength;
(3) expanded polypropylene of high fondant-strength and water are mixed to 5-10min in super mixer, prepare the jellyfish grain of different moisture content, emit stand-by.
The preparation method of the low smell glass fiber reinforced polypropylene composite material described in 12. claim 1 ~ 11 any one, is characterized in that: comprise the following steps:
(1) take by weight percentage acrylic resin, compatilizer, mineral filler and auxiliary agent and in high mixer, mix 1-3min; Mix, obtain Preblend;
(2) Preblend is placed in to the main spout of twin screw extruder, from side spout, adds jellyfish grain, glass fibre also, from the side spout feeding of forcing machine, melt extrudes, and granulating and drying, obtains.
The preparation method of 13. low smell glass fiber reinforced polypropylene composite materials according to claim 12, it is characterized in that: described in the processing conditions that melt extrudes be: a district temperature 210-230 ℃, two district temperature 220-240 ℃, three district temperature 220-240 ℃, four district temperature 220-240 ℃, five district temperature 230-250 ℃, six district temperature 240-260 ℃, seven district temperature 230-250 ℃, eight district temperature 220-240 ℃, nine district temperature 200-220 ℃, engine speed 250-600 rev/min.
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